Proton-selective 17O-1H distance measurements in fast magic-angle-spinning solid-state NMR spectroscopy for the determination of hydrogen bond lengths
Proton-selective 17O-1H distance measurements in fast magic-angle-spinning solid-state NMR spectroscopy for the determination of hydrogen bond lengths
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DOI：
10.1021/ja065415k
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发表时间：
2006-11-22
影响因子：
15
通讯作者：
Kentgens, Arno P. M.
中科院分区：
文献类型：
--
作者：
Brinkmann, Andreas;Kentgens, Arno P. M.
我们提出了一种质子选择性的方法，通过快速魔角旋转固态NMR光谱来确定有机，生物和仿生材料中的17O −1H距离。这种方法可以选择性地测定特定（17 O，1H）自旋对之间的核间距。它使得在存在共享相同17 O位点的短程17 O −1H接触的情况下，能够估计跨氢键的中程17 O···1H距离。该方法采用了新开发的基于射频脉冲序列SR 应用于质子以实现异质偶极再耦合，同时解耦同质质子偶极相互作用。快速MAS（50 kHz）和高静磁场（18.8 T）可实现所需的质子光谱分辨率。
We present a proton-selective method to determine17O−1H distances in organic, biological, and biomimetic materials by fast magic-angle-spinning solid-state NMR spectroscopy. This method allows the determination of internuclear distances between specific (17O,1H) spin pairs selectively. It enables the estimation of medium-range17O···1H distances across hydrogen bonds in the presence of short-range17O−1H contacts sharing the same17O site. The method employs the newly developed symmetry-based radiofrequency pulse sequence SR applied to the protons to achieve heteronuclear dipolar recoupling, while simultaneously decoupling the homonuclear proton dipolar interactions. Fast MAS (50 kHz) and high static magnetic fields (18.8 T) achieve the required proton spectral resolution.